EP2402473B1 - Procédé de fabrication d'un composant monocristallin constitué d'un superalliage à base de nickel - Google Patents

Procédé de fabrication d'un composant monocristallin constitué d'un superalliage à base de nickel Download PDF

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Publication number
EP2402473B1
EP2402473B1 EP11171088.5A EP11171088A EP2402473B1 EP 2402473 B1 EP2402473 B1 EP 2402473B1 EP 11171088 A EP11171088 A EP 11171088A EP 2402473 B1 EP2402473 B1 EP 2402473B1
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Prior art keywords
temperature
component
stage
nickel
cooling
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Not-in-force
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EP11171088.5A
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German (de)
English (en)
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EP2402473B8 (fr
EP2402473A3 (fr
EP2402473A2 (fr
Inventor
Mohamed Youssef Nazmy
Claus Paul Gerdes
Andreas KÜNZLER
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Ansaldo Energia Switzerland AG
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General Electric Technology GmbH
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting

Definitions

  • the invention relates to the field of materials technology. It relates to a method for producing a single-crystal component consisting of a nickel-base superalloy or directionally solidified component having comparatively large dimensions. With the aid of the method according to the invention, particularly good properties, in particular very good fatigue strength, are achieved with low-cycle stress on the component.
  • Single-crystal components made of nickel-based superalloys have, among other things, a very good material strength at high stress temperatures, but also good corrosion and oxidation resistance as well as good creep resistance. Due to these properties, when using such materials z. As in gas turbines, the inlet temperature of the gas turbine can be increased, whereby the efficiency of the gas turbine plant increases.
  • the first type to which the present invention relates may be completely solution annealed so that the entire ⁇ 'phase is in solution.
  • This is the case for example for the known alloy CMSX4 with the following chemical composition (in% by weight): 5.6 Al, 9.0 Co, 6.5 Cr, 0.1 Hf, 0.6 Mo, 3 Re, 6.5 Ta, 1.0 Ti, 6.0 W, Rest Ni or the alloy PWA 1484 with the following chemical composition (in% by weight): 5 Cr, 10 Co, 6 W, 2 Mo, 3 Re, 8.7 Ta, 5.6 Al, 0.1 Hf and the known alloy MC2, which unlike the abovementioned alloys, it is not alloyed with rhenium and has the following chemical composition (in% by weight): 5 Co, 8 Cr, 2 Mo, 8 W, 5 Al, 1.5 Ti, 6 Ta, balance Ni.
  • a typical standard heat treatment for CMSX4, for example, is the following: solution annealing at 1320 ° C / 2h / shielding gas, fan cooling.
  • the second type of single crystal nickel base superalloys is not fully heat treatable, i.
  • the entire portion of the ⁇ '-phase in a solution annealing goes into solution, but only a certain part.
  • This is the case, for example, with the known superalloy CMSX186 having the following chemical composition (in% by weight): 0.07 C, 6 Cr, 9 Co, 0.5 Mo, 8 W, 3 Ta, 3 Re, 5.7 Al, 0.7 Ti, 1.4 Hf, 0.015 B, 0.005 Zr, balance Ni and the alloy CMSX486 with the following chemical composition (in% by weight): 0.07 C, 0.015 B, 5.7 Al, 9.3 Co, 5 Cr, 1.2 Hf, 0.7 Mo, 3 Re, 4.5 Ta, 0.7 Ti, 8.6 W, 0.005 Zr, balance Ni.
  • the nickel-based superalloys of the second type are usually subjected to a two-stage heat treatment (aging process at lower temperatures), as at higher temperatures, as typically used in the alloys of the first type for solution annealing are already reached, the melting point start temperature, and thus the alloy begins to melt undesirable.
  • the creep resistance of the first type of nickel-base superalloys is usually higher than that of the second type, provided that the alloys belong to the same generation. This is mainly due to the fact that the dissolved ⁇ 'is the main source of recoverable strength.
  • Nickel-based superalloys for single-crystal components such as. B. off US 4,643,782 . EP 0 208 645 .
  • US 5,270,123 and US 7,115,175 B2 contain alloying, eg, Re, W, Mo, Co, Cr, as well as ⁇ '-phase-forming elements, for example Al, Ta, and Ti.
  • the content of high-melting alloying elements (W, Mo, Re) in the basic matrix ( austenitic ⁇ phase) increases continuously with the increase of the stress temperature of the alloy.
  • W, Mo, Re high-melting alloying elements
  • the alloys disclosed in the above references have a high creep strength, a comparatively good LCF (low cycle fatigue fatigue) and HCF (high cycle life fatigue) properties, and a high oxidation resistance.
  • the alloy CMSX-4 US 4,643,782 when used experimentally in a gas turbine at a temperature above 1000 ° C a strong coarsening of the y 'phase, which is associated with an increase in the creeping speed of the alloy adversely.
  • a similar effect leading to the flocculation of the ⁇ '-phase also results from the solidification of nickel-based superalloys due to dendritic segregation. Especially in superalloys with a high proportion of slowly diffusing elements, such. As rhenium, the segregations of these elements can not be completely eliminated within an acceptable homogenization time. Since the ⁇ '-phase, which precipitates during cooling, has a smaller lattice constant than the ⁇ -matrix and the ⁇ / ⁇ '-lattice offset in the dendrites is larger than in the interdendritic regions, internal stresses are formed during the heat treatment, especially during cooling. This leads to a change in the ⁇ 'microstructure in that the initially cubic form of ⁇ ' changes into a stretched form of ⁇ '. This is accompanied by the deterioration of mechanical properties, eg. B. fatigue strength at low load cycles.
  • the process immediately following the casting step is carried out after a two-stage slow heating of the cast object at a final HIP temperature in the range of 1174 ° C (2145 ° F) to 1440 ° C (2625 ° F), wherein the hold time is 3.5 to 4.5 hours and the pressure is in the range of 89.6 MPa (13 ksi) to 113 MPa (16.5 ksi), that is, comparatively low.
  • the aim of the invention is to avoid the mentioned disadvantages of the prior art.
  • the invention is based on the object to provide a suitable method for the production, including heat treatment, of comparatively large single-crystal components or components with directionally solidified structure of known nickel-based superalloys, with which a microstructure can be adjusted that not for raft formation ⁇ '-phase and therefore leads to improved mechanical properties, in particular an improved fatigue life at low load cycles (LCF) of the components.
  • the method according to the invention it is possible to produce large single-crystal components or components with directionally solidified microstructure of known nickel-base superalloys, which on the one hand are free of pores and on the other hand have a microstructure in which the flocculation of the ⁇ 'phase is avoided. Therefore, the components thus produced have improved mechanical properties, in particular improved low cycle fatigue life (LCF) fatigue strength.
  • the method has the advantage that it is relatively easy to implement.
  • step A) it is advantageous if the determination of the dendrite arm spacing ( ⁇ ) according to step A) takes place by metallographic means. This is relatively easy to implement and, for example, can already be carried out prior to the method on the basis of corresponding samples,
  • the quenching rate (v1) from solution annealing temperature (T 1 ) to room temperature is greater than 70 ° C./min, because then extremely fine uniformly distributed ⁇ '-particles are obtained in the ⁇ -matrix.
  • the nickel-base superalloys CMSX4 known from the prior art with the following chemical composition (in% by weight) were used: 5.6 Al, 9.0 Co, 6.5 Cr, 0.1 Hf, 0.6 Mo, 3 Re, 6.5 Ta, 1.0 Ti, 6.0 W, balance Ni.
  • the component such as a gas turbine bucket
  • the component was poured into its mold.
  • dendritic segregations arise due to the composition, in particular the comparatively high Re content.
  • Rhenium is a very slowly diffusing element, so these segregations can not be completely eliminated in the subsequent solution annealing process within an acceptable homogenization time. Since the ⁇ '-phase, which precipitates during cooling, has a smaller lattice constant than the ⁇ -matrix and the ⁇ / ⁇ '-lattice offset in the dendrites is larger than in the interdendritic regions, internal stresses are formed during the heat treatment, especially during cooling. This leads to a degradation in the ⁇ '-microstructure, in that the initially cubic form of ⁇ 'changes into a stretched form of ⁇ '. This is accompanied by the deterioration of mechanical properties, eg. B. fatigue strength at low load cycles.
  • mechanical properties eg. B. fatigue strength at low load cycles.
  • the dendrite arm spacing ⁇ is therefore first determined in different, for example, the critical regions of the cast component. This can z. B. done by metallographic way, where appropriate, this distance is already determined prior to the process on the basis of corresponding pre-cast samples.
  • the slowest diffusion element in the composition of the respective nickel base superalloy is identified to determine the diffusion coefficient D.
  • this element is rhenium, as already explained above.
  • this element is Mo.
  • the required time t is calculated at which the component at solution annealing temperature T 1 , which is lower on the one hand than the starting melt temperature T mi , and on the other hand high enough to in the necessary heat treatment window must be held so that the microsegregation of this slowest diffusion element is reduced to ⁇ 5%.
  • Fig. 1 is the time-temperature diagram of the subsequent to the casting process treatment method for producing the single crystal component from the above superalloy shown schematically.
  • the solution annealing (process step D)) of the cast component in the present embodiment thus comprises heating the component to the above solution annealing temperature T 1 of 1290-1310 ° C, holding at this temperature with the time t calculated above (4-6 h) and a rapid quenching from the solution annealing temperature T 1 to room temperature at a rate v1 ⁇ 50 ° C / min, in order to obtain very fine uniformly distributed ⁇ 'particles in the ⁇ matrix after quenching (Scheme Fig. 2a ).
  • the quenching rate is greater than 70 ° C / min, because then a microstructure is obtained with extremely fine uniformly distributed ⁇ '-particles in the ⁇ -matrix.
  • a two-stage precipitation treatment for precipitating the ⁇ '-phase is carried out at lower temperatures T 2 and T 3 in comparison to T 1 (method step E)), wherein in the first stage of the precipitation treatment a HIP method with one pressure p greater than 160 MPa and a cooling rate v2 ⁇ 50 ° C / min is applied.
  • the final temperature of the HIP process in the present embodiment is 1150 ° C, the holding time 4-6 h.
  • the applied final pressure during the HIP process is relatively high, it is greater than the internal stresses caused by the inhomogeneities in the microstructure.
  • this method step advantageously closes any micropores present in the microstructure and, on the other hand, eliminates stresses which are caused by the rapid cooling of the solution annealing temperature T 1 to room temperature or by any residual inhomogeneities in the microstructure. This prevents directional flocculation of the ⁇ 'phase by the formation of the aforementioned cubic ⁇ ' particles in the ⁇ matrix.
  • the microstructure present after the HIP-treatment step consists of fine uniformly distributed cubic ⁇ '-particles in the ⁇ matrix and is schematically in orientation Fig. 2b shown.
  • the first stage of process step E ie the HIP process, as in Fig. 3c is shown to perform.
  • the isostatic discharge pressure p is here in turn applied abruptly at the beginning of the warm-up phase, and kept constant over the entire warm-up phase, the holding phase at T 2 and in addition over the entire cooling phase. Only then, when the component has assumed room temperature, the isostatic pressure load is abruptly removed.
  • the single-crystal component / directionally solidified component is heated to a temperature T 3 of 870 ° C., held at this temperature T 3 for 16-20 h and then cooled to room temperature at a cooling rate v3 of approx. 50 ° C./minute ,
  • the end structure according to the present invention formed after this last treatment step is schematically for the ⁇ 001> orientation in FIG Fig. 2c shown.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Turbine Rotor Nozzle Sealing (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Claims (4)

  1. Procédé de fabrication d'un composant monocristallin constitué d'un superalliage à base de nickel, ou d'un composant à solidification directionnelle, dans lequel le composant est d'abord, d'une manière connue, versé dans un moule avec formation d'une structure présentant des dendrites, et dans lequel on procède ensuite à un recuit de mise en solution pour homogénéiser la structure de coulée du composant, ainsi qu'un traitement thermique de précipitation en deux étapes, caractérisé par les étapes suivantes :
    A) détermination de la distance entre les branches dendritiques (λ) dans différentes zones du composant coulé,
    B) identification de l'élément de diffusion le plus lent dans la composition de chaque superalliage à base de nickel, pour déterminer le coefficient de diffusion (D),
    C) calcul du temps (t) requis, nécessaire pour réduire à ≤ 5 % la ségrégation de l'élément de diffusion le plus lent, à une température (T1) de recuit de mise en solution d'une part inférieure à la température de fusion initiale (Tmi), mais d'autre part suffisamment élevée pour se situer dans la fenêtre de traitement thermique nécessaire,
    D) recuit de mise en solution du composant coulé, comprenant un échauffement du composant à la température (T1) de recuit de mise en solution, un maintien à cette température (T1) pendant le temps (t) calculé lors de l'étape C), et un refroidissement brusque, de la température (T1) à la température ambiante (RT) à une vitesse (v1) ≥ 50°C/min,
    E) mise en oeuvre du traitement de précipitation en deux étapes pour provoquer la précipitation de la phase γ' aux températures (T2) et (T3), qui chacune sont plus basses, après l'étape D), auquel cas, lors de la première étape du traitement de précipitation, est mis en oeuvre un procédé HIP sous une pression isostatique (p) supérieure à 160 MPa à une température de maintien (T2), et un refroidissement ultérieur de la température (T2) à la température ambiante (RT), à une vitesse de refroidissement (v1) ≥ 50°C/min, et, dans la deuxième étape, ultérieure, du traitement de précipitation, est mis en oeuvre un traitement thermique du composant à une température de maintien (T3), et un refroidissement subséquent de la température (T3) à la température ambiante (RT), à une vitesse de refroidissement (v3) de 10 à 50°C/min.
  2. Procédé selon la revendication 1, caractérisé en ce que la détermination de la distance (λ) entre les branches dendritiques selon l'étape A) a lieu par des moyens métallographiques.
  3. Procédé selon la revendication 1, caractérisé en ce que la vitesse (v1) de refroidissement brusque selon l'étape D) est > 70°C/min.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que, pour un superalliage à base de nickel ayant la composition chimique suivante (indications en % en poids) : 5,6 Al, 9,0 Co, 6,5 Cr, 0,1 Hf, 0,6 Mo, 3 Re, 6,5 Ta, 1,0 Ti, 6,0 W, le reste Ni, on met en oeuvre l'étape de recuit de mise en solution avec les paramètres suivants : 1290-1310°C/4-6 h/refroidissement rapide à v1 ≥ 50°C/min, l'opération de la première étape du traitement de précipitation γ' comprend un processus HIP sous une pression isostatique (p) > 160 MPa à une température de maintien (T2) de 1150°C et un temps de maintien de 4-8 h, et on procède à un refroidissement rapide à (v1) ≥ 50°C/min, et la deuxième étape du traitement de précipitation γ' comprend un échauffement et un maintien à 870°C/16-20 h/ainsi qu'un refroidissement à une vitesse (v3) de 10-50°C/min.
EP11171088.5A 2010-06-30 2011-06-22 Procédé de fabrication d'un composant monocristallin constitué d'un superalliage à base de nickel Not-in-force EP2402473B8 (fr)

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CH01058/10A CH703386A1 (de) 2010-06-30 2010-06-30 Verfahren zur Herstellung einer aus einer Nickel-Basis-Superlegierung bestehenden Einkristallkomponente.

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EP2402473A2 EP2402473A2 (fr) 2012-01-04
EP2402473A3 EP2402473A3 (fr) 2013-10-30
EP2402473B1 true EP2402473B1 (fr) 2017-04-26
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DE102013008396B4 (de) 2013-05-17 2015-04-02 G. Rau Gmbh & Co. Kg Verfahren und Vorrichtung zum Umschmelzen und/oder Umschmelzlegieren metallischer Werkstoffe, insbesondere von Nitinol
JP6528926B2 (ja) 2014-05-21 2019-06-12 株式会社Ihi 原子力施設の回転機器
CN105689719A (zh) * 2016-02-17 2016-06-22 西南交通大学 一种合金液滴沉积的冷却速率计算方法
DE102016202837A1 (de) * 2016-02-24 2017-08-24 MTU Aero Engines AG Wärmebehandlungsverfahren für Bauteile aus Nickelbasis-Superlegierungen
WO2018111566A1 (fr) * 2016-12-15 2018-06-21 General Electric Company Procédés de traitement pour articles en superalliage et articles associés
CN110760770B (zh) * 2019-10-30 2020-10-23 西安交通大学 单晶镍基高温合金冷变形后的热处理方法
FR3121453B1 (fr) * 2021-04-02 2023-04-07 Safran Superalliage a base de nickel, aube monocristalline et turbomachine
CN113930697B (zh) * 2021-09-23 2022-09-27 鞍钢集团北京研究院有限公司 一种750-850℃级变形高温合金的热处理方法
CN114038522A (zh) * 2021-11-18 2022-02-11 成都先进金属材料产业技术研究院股份有限公司 Gh5188合金均匀化热处理工艺的确定方法
CN114737081B (zh) * 2022-04-06 2023-03-24 暨南大学 一种具有分层微观结构的Ni-Al-Ti基高温合金及其制备方法

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Publication number Publication date
JP5787643B2 (ja) 2015-09-30
EP2402473B8 (fr) 2017-07-26
US8435362B2 (en) 2013-05-07
CH703386A1 (de) 2011-12-30
EP2402473A3 (fr) 2013-10-30
EP2402473A2 (fr) 2012-01-04
JP2012012705A (ja) 2012-01-19
US20120000577A1 (en) 2012-01-05

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